The purpose of this work was to develop a simple and rapid method to determine the radiochemical purity of 99mTc-bicisate. METHODS A rapid paper chromatographic (PC) method was developed to determine the radiochemical purity of 99mTc-bicisate and compare the results with those of the manufacturer's recommended method. The present PC method included Whatman 3MM paper as the solid phase and ethyl acetate as the solvent. RESULTS The time for chromatography by this technique was 4-5 min compared to about 23 min by the manufacturer's method. The Rf value of 99mTc-bicisate (Rf = 0.9-1.0) was widely different from those of 99mTcO4- and reduced 99mTc (Rf = 0.0 for both) so the chromatographic strip after development could be readily cut into two segments, in order to determine the labeling yield. CONCLUSIONS No significant difference in labeling yields was found between the present method and the manufacturer's method. The PC method using Whatman 3MM paper and ethyl acetate is a simple and fast technique to determine the radiochemical purity of 99mTc-bicisate and may be substituted for the manufacturer's recommended method to save time.